Recycling Blends of Hdpe and Coconut Shells as Reducing Agent for the Production of Metallic Iron From Iron Oxide Fe2o3

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INTERNATIONAL JOURNAL OF SCIENTIFIC & TECHNOLOGY RESEARCH VOLUME 3, ISSUE 1, JANUARY 2014 ISSN 2277-8616

40IJSTR©2013www.ijstr.org

Recycling Blends Of HDPE And Coconut Shells AsReducing Agent For The Production Of Metallic

Iron From Iron Oxide (Fe2O3)James Ransford Dankwah

Abstract: Laboratory studies on the production of metallic iron from iron oxide using blends of coconut shells ( cocos nucifera) and high densitypolyethylene (HDPE) as reducing agent have been performed through experiments conducted in a horizontal resistance heating tube furnaceComposite pellets were formed from mixtures of iron oxide and carbonaceous materials consisting of chars of coconut shells (CNS), HDPE and threeblends of CNS-HDPE. The iron oxide-carbonaceous material composites were heated very rapidly in a laboratory scale horizontal tube furnace at 1500°C in a continuous stream of pure argon and the off gas was analysed continuously using an infrared (IR) gas analyser and a gas chromatographic (GCanalyser equipped with a thermal conductivity detector (TCD). Elemental analyses of samples of the reduced metal were performed chemically for itscarbon and oxygen contents using a LECO carbon/sulphur and LECO oxygen/nitrogen analysers, respectively. The extent of reduction after ten minutesand the level of carburisation were determined for each carbonaceous reductant. The results indicate that metallic iron can be produced effectively fromiron oxides using CNS, HDPE and blends of these carbonaceous materials as reductants. It was revealed that the extent of reduction improvedsignificantly when CNS was blended with HDPE. The results also revealed that blending of the carbonaceous materials has a beneficial effect on theenvironment through decreasing carbon dioxide emissions.

Index Terms: Coconut shells, High density polyethylene, Composite pellets, Infrared gas analyser, Gas chromatographic analyser, LECOcarbon/sulphur analyser, LECO oxygen/nitrogen analyser, Extent of reduction, Carburisation

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1 INTRODUCTION

23% of HDPE was recycled in Australia in 2011-2012 [1]. Therest was either landfilled or dumped illegally. This category ofwaste stream occupies large landfill space and is notbiodegradable. HDPE, a thermoplastic polymer contains highlevels of carbon and hydrogen and its thermal decompositionat high temperatures generates large amounts of the gaseousreducing species H2 and CH4 [2], which are known reductantsof metal oxides. CNS is a cheap and abundantly availablesolid waste material that is cultivated in several parts ofGhana, especially along the coastal belts. As a biomassmaterial, it is a renewable fuel and generally considered as a

‘carbon neutral fuel’. The use of waste polymeric materials aschemical feedstock in iron and steelmaking is currently gainingthe attention of researchers. As a means of recycling wasteplastics, low temperature pyrolysis along with combustion andthermal degradation (of coal, plastics, biomass and theirblends) has been widely investigated by various researchers[3], [4], [5], [6], [7], [8], [9], [10], [11], [12]. However, not muchis known about the use of blends of CNS/HDPE as reductantsor carburisers in iron and steelmaking technologies. In thepresent work, the potential for producing metallic iron fromhematite using blends of CNS and HDPE as reducing andcarburising agents is investigated under inert atmosphere in acustom made horizontal tube furnace.

2 EXPERIMENTAL

2.1 Raw MaterialsCNS (collected from Koforidua, Ghana) and its blends in threedifferent proportions (Fig. 1) with granulated HDPE (obtainedfrom Qenos Pty. Ltd., Victoria, Australia) were employed in thisstudy as carbonaceous materials. The chemical composition(wt %) of the samples and the ash analyses are given inTables 1- 3. Pulverised reagent grade iron oxide (assaying96.89% Fe2O3) was obtained from Ajax FineChem Pty LtdTaren Point, NSW, Australia; its composition (determined byXRF analysis) is given in Table 4.

Fig. 1: Blend compositions of the different carbonaceousmaterials utilised in this study

Samples of CNS were ground and sieved to particle size in therange of -470 +450 µm while samples of granulated HDPEwere crushed to smaller sizes by using a cutting mil“Pulverisette 15” (Fritsch GmbH, Idar -Oberstein, Germany). Bymeans of a sieve insert with 0.5 mm trapezoidal perforations inthe cutting mill a particle size -470 +450µm, similar to that ofCNS was obtained. Blends of CNS/HDPE were prepared in

0

50

100

CNS HDPE

___________________________________

Dr. James R. Dankwah (formerly of School ofMaterials Science and Engineering, UNSW, Sydney,

Australia) is currently a lecturer in Ferrous Metallurgyat University of Mines and Technology, Tarkwa,Ghana, PH-+233 205 802 944.E-mail: [email protected]

mailto:[email protected]








(a)

three different proportions.

TABLE 1: ELEMENTAL ANALYSIS OF HDPE AND CNS

Component C H S N O*

HDPE (wt %) 85.5 14.2 0.3 - -

CNS Raw (wt %) 52.4 5.72 0.03 0.11 41.77

CNS Char (wt %) 78.1 3.49 0.01 0.15 17.55

* By difference

TABLE 2: PROXIMATE ANALYSES OF HDPE AND CNS

Component Moisture Ash*Volatilematter*

Fixedcarbon*

HDPE (wt %) - 0.3 99.7 -

Raw (wt %) 8.5 0.87 87.5 11.6

Char (wt %) 5.40 0.70 29.80 69.60

*Dry basis

TABLE 3: ASH ANALYSIS OF RAW CNS

Component Raw (wt %)

SiO2 37.5

Fe2O3 1.8

Al2O3 1.8

TiO2 0.29

P2O5 3.1

Mn3O4 0.07

CaO 6.2

MgO 4.2

Na2O 3.7

K2O 23.2

SO3 5.2

V2O5 1.7

ZnO 2.4

BaO 0.56

SrO 0.12

TABLE 4: ELEMENTAL ANALYSIS OF HDPE AND CNS

Component Composition (wt %)Fe2O3 96.89

SiO2 0.445

CaO 0.0225

MnO 0.020

ZnO 0.0115

TiO2 0.134

SO3 0.257

LOI 2.22

2.2 Thermal Decomposition StudiesPulverised HDPE sample (particle size below 1 mm) wasmixed thoroughly with alumina powder and cylindrical pelletswere formed from the resulting mixture by applying a load of7.5 tonnes for 1 minute in a hydraulic press. The use of thealumina powder was to slow down the decomposition process(to enable gas measurements by the IR-analyser) as well as

mimic the reduction environment through the cylindricapellets. The alumina powder acted as a blank medium, sinceits reduction will be difficult at the selected temperature. Theexperimental apparatus consisted of two gas analysersconnected to an electrically heated horizontal tube furnaceand a data logging computer (Fig. 4). CO, CO2 and CH4 weremonitored continuously by an IR gas analyser (AdvanceOptima model ABB^® AO2020) while a GC analyser (SR8610C Multiple Gas Chromatograph #3 configurationequipped with a thermal conductivity detector, TCD) monitoredO2, H2, H2O and CnHm.

Fig. 2: Composite pellet (of Al2O3 + HDPE) utilized for thermadecomposition of HDPE at 1550 °C

The furnace was purged continuously with argon gas(99.995% purity) to ensure an inert atmosphere. The furnace

was preheated to the desired temperature and the sample wasinserted; gas measurement commenced immediately afteinsertion and continued for 900 s. No appreciable change ingas composition was observed beyond 900 s.

2.3 Reduction StudiesThe reduction experiments were conducted in a similar way asthe thermal decomposition process, except that compositepellets in this case contained iron oxide instead of aluminaAbout 1.86 g of iron oxide was subsequently mixed with thecarbonaceous blends (~ 30 wt %) and compacted in a die toproduce cylindrical pellets (~ 14 mm thick and 15 mmdiameter) (Fig. 3d), by applying a load of 7.5 tonnes for 120 sin a hydraulic press.

(b)





Fig. 3: (a) HDPE, (b) iron oxide, (c) CNS (raw) and (d)cylindrical pellet of iron oxide-HDPE

Fig. 4: Schematic of the horizontal tube furnace and IR gasanalyser system. (1 Sample Rod; 2 Alumina tube; 3 Reaction mixture;4 PC; 5 DVD; 6 CCD Camera; 7 Hot Zone; 8 Cold Zone; 9 Gas analyser;10 Quartz window; 11 Thermocouple; 12 Argon gas)

Reacted carbonaceous material/iron oxide samples werequenched by rapidly withdrawing the tray from the hot zoneinto the cold zone of the furnace. Particles of reduced ironmetal, which were clearly visible to the naked eye, wereremoved by a magnetic screw driver and its content wasdetermined by the following chemical analysis methods:

LECO Carbon/Sulphur analyser (model CS 230,LECO Corporation, Michigan, USA) for its C contentand

LECO Nitrogen/Oxygen analyser (model TC-436 DR602-500-600, LECO Corporation, Michigan, USA) forits O content.

2.4 Proposed Mechanism of Reduction of Iron Oxideby Biomass/Plastics Blend

The reactions that take place in the furnace may beconveniently divided into the following four categories:

1) Conversion of the polymer into methane and otherhydrocarbons.

Polymer →CnHm (g) 1 2) Thermal decomposition of methane (and otherhydrocarbons) into carbon and hydrogen or reformation intoCO and H2:

CnHm (g) = n C (s) + (m/2) H2 (g) 2a

CnHm (g) + n CO2 (g) = 2n CO (g) + (m/2) H2 (g) 2b

CnHm (g) + n H2O(g) = n CO (g) + (n + m/2) H2 (g) 2c

3) Reduction of Fe2O3 by hydrogen, carbon and carbonmonoxide to produce Fe3O4:

Fe2O3 + ⅓H2 = ⅔Fe3O4 + ⅓H2O 3a

Fe2O3 + ⅓C = ⅔Fe3O4 + ⅓CO 3b

Fe2O3 + ⅓CO = ⅔Fe3O4 + ⅓CO2 3c

4) Reduction of Fe3O4 by hydrogen, carbon and carbonmonoxide to produce FeO

Fe3O4 + H2 = 3FeO + H2O 4a

Fe3O4 + C = 3FeO + CO 4b

Fe3O4 + CO = 3FeO + CO2 4c

5) Reduction of FeO by hydrogen, carbon and carbonmonoxide to produce Fe

FeO + H2 = Fe + H2O 5a

FeO + C = Fe + CO 5b

FeO + CO = Fe + CO2 5c

6) Auxiliary reactions 13, 14)

i. Water gas shift reaction:

H2O (g) + CO (g) = H2 (g) + CO2 (g) 6

ii. Gasification of C by H2O:

H2O (g) + C (s) = H2 (g) + CO (g) 7

iii. Gasification of C by CO2 (Boudouard reaction):

CO2 (g) + C (s) = 2CO (g) 8

iv. Carbon dissolution into molten metal:

(c)

(d)





C (s) = C 9

3 RESULTS AND DISCUSSIONS

3.1 Thermal Decomposition Behaviour of HDPE at1500°C

The gas generation behaviour during the thermaldecomposition of HDPE-alumina at 1500 °C is illustrated in

Fig. 4. The predominant gases from the thermaldecomposition of HDPE are the reducing gases CH4 and H2 (peak identified in Fig. 5). Minor amounts of CO and CO2 weredetected as indicated in Fig. 4. As alumina was unlikely tohave been reduced by HDPE (and the HDPE had no oxygen),the only probable source of CO and CO2 could be from partialoxidation of the HDPE by trapped oxygen in the pores of theHDPE-alumina compact and/or minor reformation of CH4 byH2O and/or CO2 (equations 10-12).

½(C2H4)n + O2 = nCO2 + nH2O 10

CH4 + CO2 = 2CO + 2H2 11

CH4 + H2O = CO + 3H2 12

However, the contents of CO and CO2 were negligiblecompared to H2 and CH4 when HDPE-alumina was heated at1500 °C.

Fig. 4: Gas generation behaviour during the thermaldecomposition of HDPE from a HDPE-alumina compact

Fig. 5: Gas chromatogram obtained after 60 s of heatingHDPE-alumina compact

Direct ingress of oxygen into the furnace was unlikely as thefurnace was purged continuously with argon. After 60 s oheating the compact, the area ratio H2 /CH4 was approximately1.0 but this gradually increased to about 2.5 after 300 simplying that CH4 undergoes cracking to generate more Hand nascent C in the course of heating, probably throughequation 13, which is spontaneous above 550 °C.

CH4 = C + 2H2 ΔG° = 91,040 – 110.7 T [J mol-1

] 13

It is clear from Figs 4 and 5 that the main reductants producedfrom the thermal decomposition of HDPE are H2, CH4, andminor amounts of CO and C. The generated carbon particlesare present at the Nano-scale level. The potential for HDPE tofunction as a reductant for iron oxide reduction thereforeexists, as indicated by the formation of Nano-scale solidcarbon and gaseous H2 and CH4.

3.2 Nature of Metal ProducedSamples of reduced metal were obtained for all blend proportionsand the result for HDPE as the reducing agent is shown in Fig. 6The vigorous nature of the reaction is apparent from Fig. 6, where

several small droplets of metallic iron are seen distributed acrossthe entire volume of the crucible.

Fig. 6: Droplets of metallic iron and char obtained after 600seconds of reduction of iron oxide by a) HDPE and b) CNS

The particles could not coagulate into one big lump because othe excess amount of carbonaceous materials (1.45 ≤ C/O ≤1.68) utilised in this investigation, the essence of which was toensure that enough carbonaceous material was available for thereaction to go to completion.

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C o n c n

o f C H 4

( V o l % )

Time (s)

CH4

CO

CO2

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I n t e n s i t y ( A r b i t r a r y U n i t s )

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CH4CO CO2

b)

a)

Reduced metal

Reduced metal





3.3 IR Gas AnalysesThe contents of CO and CO2 in the off-gas were measuredcontinuously by an IR gas analyser from which the rates of gasevolution (µmol/s.g-Fe) were calculated for each carbonaceousblend. The results are shown in Fig. 7. The rates of evolution ofCO and CO2 increase slowly for the first 200 seconds for HDPE(Fig. 7a), followed by a sharp rise, attaining maximum values of154.4 and 16.6 µmol/s.g-Fe after about 230 and 220 seconds,

respectively. Fig. 7b illustrates the gas generation behaviour ofCNS. Active gas generation commences after 180 seconds, andattains maximum values of 96.7 and 26.4 µmol/s.g-Fe after about330 and 210 seconds for CO and CO2, respectively. CO2 generation for CNS is quite significant, unlike HDPE, which hasalmost negligible generation. Gas generation for HDPE-CNSblends (Figs. 7c-e) commenced earlier than HDPE or CNS,indicating that blending promotes gasification and/or reduction ofiron oxide. It is apparent from Fig. 7 that all the blends showedlower CO2 evolution compared to CNS. The relatively low valuesrecorded for CO2 compared to CO may be an indication of directreduction of Fe2O3 by C or a dominant carbon gasification by CO2 (Boudouard reaction, equation 8) and/or by water (equation 7).Equations 7 and 8 are highly endothermic and occur above 1000

°C 15). Another possible reaction is the direct reduction of Fe2O3 by CH4, which was the predominant gaseous hydrocarbondetected in the off-gas in the initial stages of the reaction.

3CH4 + Fe2O3= 2Fe + 6H2 + 3CO (14)

Fig. 7: Change in the rate of generation of CO and CO2 withtime for each carbonaceous reductant

3.2 Extent of ReductionThe extent of reduction (after 600 s) was calculated from theoxygen content of the reduced metal produced from the reactionof the iron oxide with each carbonaceous reductant. The results

are shown in Table 5.

TABLE 5: EXTENT OF REDUCTION ATTAINED AFTER 600 S OF

REDUCTION OF Fe2O3 WITH VARIOUS CARBONACEOUS REDUCTANTS

Carbonaceous Reductant

CNS Blend A Blend B Blend C HDPE

Extent ofreduction (%)

73.9 79.6 82.8 86.8 84.7

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Time (s)

rCO

rCO2

a) HDPE

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G a s g e n e r a

t i o n r a t e ( µ m o l / s . g - F e )

Time (s)

rCO

rCO2

b) CNS

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t i o n r a t e ( µ m o l / s . g - F e )

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rCO2

c) Blend A

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rCO2

d) Blend B

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rCO2

e) Blend C





Blending of CNS with HDPE resulted in improved extent ofreduction because more hydrogen was released into the reactionsystem as indicated by the improved peak of hydrogen in thechromatogram of HDPE compared to that of CNS (Fig. 8). Thisresults in an increase in the H2 /CO ratio in the system. Work doneby Alamsari et al. [16] has shown a significant improvement iniron oxide reduction with an increase in the H2 /CO ratio. Similarobservations were reported by other researchers [17], [18], [19].

Fig. 8: Gas chromatogram obtained after reduction of ironoxide by (a) HDPE and (b) CNS for 1 minute at 1500 °C

3.3 Environmental Considerations: CO2 emissionThe rate of CO2 generation in the first ten minutes by eachcarbonaceous reductant is plotted in Fig. 9 whilst theaccumulated amount of CO2 generated (µmol) is shown in Fig.10. It is clear from Figs (9 and 10) that the highest rate (26.4µmol/g.s Fe) and highest accumulated amount (~3257 µmol) ofCO2 was produced from the reaction involving CNS. Blending ofCNS with HDPE resulted in a decrease in the rate and amount of

CO2 evolved up to Blend B, which recorded the lowest rate andaccumulated amount of 11.5 µmol/g.s Fe and 853 µmol,respectively. The significantly high value of CO2 recorded for CNSas opposed to that for HDPE and the blends is attributed to thehigh oxygen content of CNS char (17.55 wt %). The observeddecrease in CO2 emissions with HDPE addition agrees with theobservation by Matsuda et al. [20] that it is possible to utilisewaste plastics to produce metallic iron without generating CO2.Singh et al. [12] observed a 6.5% reduction in CO2 emissionswhen coal was fired with 25% HDPE (measured in terms ofthermal energy). They attributed this to the higher heating valueof HDPE (46.2 MJ/kg) compared to that of the coal.

Fig. 9: Concentration of CO2 generated by reactions of ironoxide with each carbonaceous reductant

Fig. 10: Amount of CO2 generated by reactions of iron oxidewith each carbonaceous reductants

Since biomass is considered as a CO2-neutral materialachieving further reduction in gaseous emissions throughblending with postconsumer plastics would be a great steptowards ultralow CO2 emissions in iron and steel productiontechnologies.

4 CONCLUSIONS A laboratory investigation has been conducted on thepossibility of a coke-free iron making utilising postconsumeHDPE, chars of waste CNS and their blends as reducing

agents. Major findings of this investigation are:(1) Blends of postconsumer HDPE with waste CNS couldbe used effectively as reducing agents in ironmaking.

(2) The extent of reduction after ten minutes of reactionshowed an improvement with the amount of HDPEblended with CNS.

(3) Although biomass is considered as a CO2-neutramaterial, this investigation has shown that it is stilpossible to achieve further reduction in gaseousemissions through blending the biomass withpostconsumer plastics, a measure that would be agreat step towards ultralow CO2 emissions in iron andsteelmaking technologies.

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A m o u n t o f C O 2 g e n e r a t e d ( µ m o l )

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HDPE

CS

Blend A

Blend B

Blend C

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H a y e s e p p

c o l u m n(a) HDPE

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CH4CO CO2

H2O

(b) CNS

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Blend A

Blend B

Blend C




46IJSTR©2013ij

ACKNOWLEDGMENT Part of this work was done at the School of Materials Scienceand Engineering, UNSW, Sydney, Australia. I am grateful toProf Veena Sahajwalla (SMaRT@UNSW) and Dr PramodKoshy for fruitful discussions.

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[13] J.R. Dankwah, P. Koshy, N.M. Saha-Chaudhury, P. O'Kane, C.

Skidmore, D. Knights, and V. Sahajwalla, “Reduction of FeO inEAF steelmaking slag by metallurgical coke and waste plasticsblends”, ISIJ Int., vol. 51, no. 3, p. 498-507, 2011

[14] D. Gosh, A.K. Roy, and A. Gosh, “Reduction of ferric oxidepellets with methane”. ISIJ Int., vol. 26, pp. 186-193, 1986

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[18] A.A. El-Geassy and V. Rajakumar, “Gaseous reduction owustite with H2, CO and H2-CO mixtures”, Trans. ISIJ, vol. 25pp. 449-458, 1985

[19] A. Pineau, N. Kanari, and I. Gaballah, “Kinetics of reduction oiron oxides by H2. Part I: low temperature reduction of hematite”Thermochim. Acta, vol. 447, pp. 89-100, 2006

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Documents

Recycling Blends of Hdpe and Coconut Shells as Reducing Agent for the Production of Metallic Iron From Iron Oxide Fe2o3